Search results for "Elution"
showing 10 items of 337 documents
Prediction of Peak Shape and Characterization of Column Performance in Liquid Chromatography as a Function of Flow Rate
2015
Traditionally, column performance in liquid chromatography has been studied using information from the elution of probe compounds at different flow rates through van Deemter plots, which relate the column plate height to the linear mobile phase velocity. A more recent approach to characterize columns is the representation of the peak widths (or the right and left peak half-widths) for a set of compounds versus their retention times, which, for isocratic elution, give rise to almost linear plots. In previous work, these plots have been shown to facilitate the prediction of peak profiles (width and asymmetry) with optimization purposes. In this work, a detailed study on the dependence of the …
Apparent and Real Distribution in GPC (Experiments with PMMA Samples)
1971
Abstract Molecular weight distribution curves obtained by GPC are broadened if concentration and flow rate are fixed in the usual range. Therefore, the apparent nonuniformity U app of the samples is larger than the real non-uniformity U = (Mw/Mn) −1. For a number of fractionated and unfractionated samples of polymethyl methacrylate we determined M n and M w by osmotic, light-scattering, and viscosity measurements. Thus, the real value of U can be compared to U app obtained by GPC at different concentrations and flow rates, υ. The excess nonuniformity U exc is evaluated as function of concentration c, polydispersity, molecular weight, and flow rate. For c = 0 and υ = 0, U exc is not far from…
HPLC determination of volatile phenols in wines
1993
An alternative to the traditional solvent extraction method used to extract and rapidly quantify ethyl-and vinylphenol and ethyl-and vinylgaiacol from wine is presented. The method is based on retention of volatile phenols on adsorbants. Among the tested resins, the most efficient, AG 2-X8 (anion exchange resin), worked as well with a synthetic solution as with wines. The percolation of clarified wine adjusted to pH 9 on this resin permits, in particular, the elimination of organic acids. Phenols are not eluted after rinsing the column with 1N HCl, but are eluted with methanol after this treatment. Good recovery (91 %) and good repeatability are observed. The eluate is directly analysed by …
Quantitative determination of sotolon in wines by high-performance liquid chromatography
1993
Sotolon (4,5-dimethyl-3-hydroxy-2(5H)-furanone) is a key flavour compound in the french flor-sherry “Vin jaune”. This compound was determined quantitatively by extraction of 25 ml of wine on a XAD-4 resin, elution with diethyl ether, separation by HPLC on a Lichrospher 100 Diol column, elution with dichloromethane/hexane (60/40) and UV detection at 232 nm. The amount of sotolon in “Vin jaune” (120 to 268 μg/l) was related to the development of the yeast film over a period of 6 years. Only 6 to 51 μg/l were found in the “Vin de paille” which is made with overmaturated grapes of the same Savagnin vine-plant but without development of yeasts, and 80 to 140 μg/l in “Tokai” which are partly grow…
An on-line system for preconcentration and determination of lead in wine samples by FAAS
2002
A flow injection method has been developed for the direct determination of free available Pb(II) and total Pb content in wine samples. The method is based on the chemical sorption of Pb(II), from pH 7 buffered solutions, on a packed polyurethane foam column, modified by addition of 2-(2-benzothiazolylazo)-p-cresol (BTAC). After this step, lead was directly eluted with a stream of 0.1 mol l(-1) HCl into an air C(2)H(2) flame in which lead was determined by atomic absorption spectrometry. Total lead was analyzed after sample digestion with nitric acid and hydrogen peroxide, being free available lead determined by direct sample on-line preconcentration and elution. The method provides a limit …
Molecularly imprinted polymer solid phase extraction of fungicides from wine samples
2014
In order to preconcentrate iprodione fungicide in white wine samples, molecularly imprinted polymers (MIPs) specific for iprodione were synthesized using two polymerization approaches: precipitation (MIPp) and bulk polymerization (MIPb). A comparison of the performance of the MIPs and the corresponding non-imprinted polymers (NIPs) was conducted in batch studies. In this case, the MIPp revealed better recognition properties toward iprodione in wine samples than the MIPb. The MIPp and MIPb were then used as sorbents on solid phase extraction cartridges (MISPEp and MISPEb consecutively) in order to pre-concentrate iprodione from white wine samples. The optimization of the MISPE elution step w…
Comparison of different sample treatments for the analysis of ochratoxin A in must, wine and beer by liquid chromatography.
2004
Abstract Ochratoxin A (OTA) is a mycotoxin produced by some species of Aspergillus and Penicillium verrucosum. It has been found in foods and feed all over the world. There is a great concern about OTA because it is nephrotoxic and probably, carcinogenic to humans. Most of analytical methods developed for OTA in wine, beer and other products are based on LC with fluorescence detection (LC–FLD). In the present work, various procedures for extraction and/or clean-up for determination of OTA in musts, wine and beer by LC–FLD were compared: (1) dilution with polyethylen glycol 8000 and NaHCO3 solution and clean-up an on immunoaffinity column (IAC); (2) extraction with chloroform and IAC clean-u…
The use of core-shell high-performance liquid chromatography column technology to improve biogenic amine quantification in wine
2015
BACKGROUND HPLC column technology has been improved, providing better resolution of closely eluting compounds, better analyte sensitivity, and shorter analysis times. The core-shell technology columns offer a faster analysis through the use of shorter columns without compromising resolution. The aim of this work was to improve the methods for determination of biogenic amines (BAs) in wine using the new HPLC PFP core-shell column technology. RESULTS Two different elution programs were designed to quantify BAs with the core-shell PFP column. Program I flow rate was 2 mL min−1. The total elution time was 10 min. In elution program II, the flow rate was 0.8 mL min−1 and the total elution time w…
Multi-scale optimisation vs. genetic algorithms in the gradient separation of diuretics by reversed-phase liquid chromatography
2019
Abstract Multi-linear gradients are a convenient solution to get separation of complex samples by modulating carefully the gradient slope, in order to accomplish the local selectivity needs for each particular solute cluster. These gradients can be designed by trial-and-error according to the chromatographer experience, but this strategy becomes quickly inappropriate for complex separations. More evolved solutions imply the sequential construction of multi-segmented gradients. However, this strategy discards part of the search space in each step of the construction and, again, cannot deal properly with very complex samples. When the complexity is too large, the only valid alternative for fi…
Gradient design for liquid chromatography using multi-scale optimization.
2017
Abstract In reversed phase-liquid chromatography, the usual solution to the “general elution problem” is the application of gradient elution with programmed changes of organic solvent (or other properties). A correct quantification of chromatographic peaks in liquid chromatography requires well resolved signals in a proper analysis time. When the complexity of the sample is high, the gradient program should be accommodated to the local resolution needs of each analyte. This makes the optimization of such situations rather troublesome, since enhancing the resolution for a given analyte may imply a collateral worsening of the resolution of other analytes. The aim of this work is to design mul…